3-bromopropyl(trichloro)silane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under a nitrogen atmosphere, (3-bromopropyl)trichlorosilane (22) (1 equiv., 5 g, 19.5 mmol) was cooled down to 0° C., then 1M allylmagnesium bromide solution (3.3 equiv., 64.5 ml) was added and stirred at room temperature for 3 hours. To the reacted mixture, diethyl ether was added and neutralized with aqueous solution of citric acid. The obtained water layer was extracted with diethyl ether and the collected organic layer was washed with saturated saline solution, then dried over anhydrous magnesium sulfate and filtered, concentrated under reduced pressure, obtaining a crude product. The crude product was passed through silica gel column chromatography (eluent: n-hexane), obtaining triallyl(3-bromopropyl)silane (23) represented by the following chemical reaction equation (yield: 5.2 g, yield (%): 98%). The obtained water layer was extracted with diethyl ether the collected organic layer was washed with saturated saline solution dried over anhydrous magnesium sulfate filtered concentrated under reduced pressure obtaining a crude product

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under a nitrogen atmosphere, (3-bromopropyl)trichlorosilane (22) (1 equiv., 5 g, 19.5 mmol) was cooled down to 0° C., then 1M allylmagnesium bromide solution (3.3 equiv., 64.5 ml) was added and stirred at room temperature for 3 hours. To the reacted mixture, diethyl ether was added and neutralized with aqueous solution of citric acid. The obtained water layer was extracted with diethyl ether and the collected organic layer was washed with saturated saline solution, then dried over anhydrous magnesium sulfate and filtered, concentrated under reduced pressure, obtaining a crude product. The crude product was passed through silica gel column chromatography (eluent: n-hexane), obtaining triallyl(3-bromopropyl)silane (23) represented by the following chemical reaction equation (yield: 5.2 g, yield (%): 98%). The obtained water layer was extracted with diethyl ether the collected organic layer was washed with saturated saline solution dried over anhydrous magnesium sulfate filtered concentrated under reduced pressure obtaining a crude product